Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (3): 273-280.DOI: 10.3724/SP.J.1123.2021.08005
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PING Hua1,2, ZHAO Fang1, LI Cheng1, WANG Beihong1, KONG Hongling1, LI Yang1, MA Zhihong1,*()
Received:
2021-08-06
Online:
2022-03-08
Published:
2022-03-04
Contact:
MA Zhihong
Supported by:
CLC Number:
PING Hua, ZHAO Fang, LI Cheng, WANG Beihong, KONG Hongling, LI Yang, MA Zhihong. Rapid and simultaneous determination of glyphosate, glufosinate, and their metabolites in soil by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2022, 40(3): 273-280.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2021.08005
No. | Compound | Compound abbr. | Retention time/min | Parent ion (m/z) | Daughter ions (m/z) | Cone voltage/V | Collision energies/eV |
---|---|---|---|---|---|---|---|
1 | glyphosate | GLY | 7.73 | 168.05 | 63.11*, 150.00 | 20 | 20, 10 |
2 | (aminomethyl)phosphonic acid | AMPA | 4.82 | 110.04 | 63.11*, 79.18 | 60 | 18, 20 |
3 | 3-(methylphosphinico)propionic acid | MPP | 6.65 | 151.06 | 63.14, 107.00* | 46 | 24, 20 |
4 | glufosinate | GLUF | 6.22 | 180.11 | 85.10*, 95.05 | 50 | 20, 18 |
5 | N-acetyl glufosinate | NAG | 6.65 | 222.09 | 134.20, 136.12* | 50 | 24, 22 |
Table 1 MS parameters for the five compounds
No. | Compound | Compound abbr. | Retention time/min | Parent ion (m/z) | Daughter ions (m/z) | Cone voltage/V | Collision energies/eV |
---|---|---|---|---|---|---|---|
1 | glyphosate | GLY | 7.73 | 168.05 | 63.11*, 150.00 | 20 | 20, 10 |
2 | (aminomethyl)phosphonic acid | AMPA | 4.82 | 110.04 | 63.11*, 79.18 | 60 | 18, 20 |
3 | 3-(methylphosphinico)propionic acid | MPP | 6.65 | 151.06 | 63.14, 107.00* | 46 | 24, 20 |
4 | glufosinate | GLUF | 6.22 | 180.11 | 85.10*, 95.05 | 50 | 20, 18 |
5 | N-acetyl glufosinate | NAG | 6.65 | 222.09 | 134.20, 136.12* | 50 | 24, 22 |
Compound | Linear range/ (μg/L) | Linear equation | r2 | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|---|
GLY | 5.0-500 | y=158.5x+488.5 | 0.9980 | 4.0 | 13.3 |
AMPA | 5.0-500 | y=60.3x+94.0 | 0.9994 | 4.0 | 13.3 |
MPP | 2.0-500 | y=144.8x+108.7 | 0.9986 | 2.0 | 6.7 |
GLUF | 2.0-500 | y=114.4x+153.1 | 0.9988 | 2.0 | 6.7 |
NAG | 2.0-500 | y=315.1x+580.4 | 0.9993 | 2.0 | 6.7 |
Table 2 Linear ranges, linear equations, correlation coefficients (r2), method LODs and LOQs of the five compounds
Compound | Linear range/ (μg/L) | Linear equation | r2 | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|---|
GLY | 5.0-500 | y=158.5x+488.5 | 0.9980 | 4.0 | 13.3 |
AMPA | 5.0-500 | y=60.3x+94.0 | 0.9994 | 4.0 | 13.3 |
MPP | 2.0-500 | y=144.8x+108.7 | 0.9986 | 2.0 | 6.7 |
GLUF | 2.0-500 | y=114.4x+153.1 | 0.9988 | 2.0 | 6.7 |
NAG | 2.0-500 | y=315.1x+580.4 | 0.9993 | 2.0 | 6.7 |
Compound | 0.02 mg/kg | 0.05 mg/kg | 0.2 mg/kg | |||||
---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | |||
AMPA | 91.2 | 0.93 | 84.7 | 4.81 | 86.6 | 1.4 | ||
MPP | 97.8 | 3.4 | 98.3 | 3.08 | 97.5 | 1.2 | ||
GLY | 74.6 | 6.8 | 74.8 | 2.02 | 74.2 | 4.9 | ||
GLUF | 101 | 2.9 | 98.7 | 3.07 | 98.3 | 2.7 | ||
NAG | 97.5 | 6.8 | 98.8 | 5.55 | 94.4 | 2.6 |
Table 3 Spiked recoveries and precisions of the five compounds in soil with low organic matter(n=6)
Compound | 0.02 mg/kg | 0.05 mg/kg | 0.2 mg/kg | |||||
---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | |||
AMPA | 91.2 | 0.93 | 84.7 | 4.81 | 86.6 | 1.4 | ||
MPP | 97.8 | 3.4 | 98.3 | 3.08 | 97.5 | 1.2 | ||
GLY | 74.6 | 6.8 | 74.8 | 2.02 | 74.2 | 4.9 | ||
GLUF | 101 | 2.9 | 98.7 | 3.07 | 98.3 | 2.7 | ||
NAG | 97.5 | 6.8 | 98.8 | 5.55 | 94.4 | 2.6 |
Compound | 0.02 mg/kg | 0.05 mg/kg | 0.2 mg/kg | |||||
---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | |||
AMPA | 92.1 | 1.6 | 110 | 1.8 | 97.5 | 5.2 | ||
MPP | 98.6 | 6.9 | 115 | 7.1 | 113 | 1.7 | ||
GLY | 114 | 3.0 | 99.1 | 5.7 | 90.8 | 7.0 | ||
GLUF | 108 | 3.9 | 104 | 6.1 | 116 | 0.40 | ||
NAG | 106 | 5.7 | 105 | 5.0 | 111 | 0.51 |
Table 4 Spiked recoveries and precisions of the five compounds in soil with high organic matter(n=6)
Compound | 0.02 mg/kg | 0.05 mg/kg | 0.2 mg/kg | |||||
---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | |||
AMPA | 92.1 | 1.6 | 110 | 1.8 | 97.5 | 5.2 | ||
MPP | 98.6 | 6.9 | 115 | 7.1 | 113 | 1.7 | ||
GLY | 114 | 3.0 | 99.1 | 5.7 | 90.8 | 7.0 | ||
GLUF | 108 | 3.9 | 104 | 6.1 | 116 | 0.40 | ||
NAG | 106 | 5.7 | 105 | 5.0 | 111 | 0.51 |
Soil source and type | Derivatization | Detection method | Compound | Linear range/ (μg/L) | LOD/ (μg/kg) | Recovery/ % | Reference | |
---|---|---|---|---|---|---|---|---|
Apple field soil (organic matter content 2.65%) | yes | GC-NPD | GLY | 100- | 20000 | 20 | 84.4-94.0 | [ |
Sri Lanka farmland | yes | GC-MS | GLY | 2- | 100 | 20 | 83.4 | [ |
AMPA | 2- | 100 | 20 | 87.1 | ||||
Mulberry field soil | yes | HPLC-UV | GLY | 5000- | 35000 | - | 98.5-103 | [ |
Peach field soil (loess soil, black soil and | yes | HPLC-MS/MS | GLY | 1- | 2000 | 10 | 76.7-93.0 | [ |
red soil) | AMPA | |||||||
Yellow cinnamon soil, lou soil and loess soil | yes | HPLC-MS/MS | GLY | 1.6- | 200 | 0.80 | 84.0-104 | [ |
(organic matter content from 0.74%-1.25%) | AMPA | 1.6- | 200 | 0.94 | 84.0-104 | |||
Red loam soil, rice soil and black soil | yes | HPLC-FLD | GLY | 10- | 500 | 20 | 68.3-109 | [ |
- | no | IC | GLY | 20.0- | 1000 | 40 | 80.2-86.4 | [ |
GLUF | 20.0- | 1000 | 80 | 87.1-101 | ||||
AMPA | 5.0- | 400 | 20 | 85.8-106 | ||||
- | no | UPLC-MS/MS | GLY | 20- | 200 | 0.5 | 79.7-96.2 | [ |
AMPA | 20- | 200 | 0.6 | 77.8-99.5 | ||||
- | no | UPLC-MS/MS | GLY | 100- | 10000 | 100 | 85.8-94.6 | [ |
- | no | UPLC-MS/MS | GLY | 10- | 1000 | 20 | 77.5-92.0 | [ |
AMPA | 10- | 1000 | 20 | |||||
GLUF | 5- | 500 | 10 | |||||
Peach field soil (organic matter content | no | UPLC-MS/MS | GLY | 5- | 500 | 4.0 | 74.2-78.8 | this |
2.89%-7.38%) | AMPA | 83.7-91.2 | method | |||||
GLUF | 2- | 500 | 2.0 | 94.1-101 | ||||
MPP | 97.5-104 | |||||||
NAG | 94.4-108 |
Table 5 Comparison of this method with other literature methods
Soil source and type | Derivatization | Detection method | Compound | Linear range/ (μg/L) | LOD/ (μg/kg) | Recovery/ % | Reference | |
---|---|---|---|---|---|---|---|---|
Apple field soil (organic matter content 2.65%) | yes | GC-NPD | GLY | 100- | 20000 | 20 | 84.4-94.0 | [ |
Sri Lanka farmland | yes | GC-MS | GLY | 2- | 100 | 20 | 83.4 | [ |
AMPA | 2- | 100 | 20 | 87.1 | ||||
Mulberry field soil | yes | HPLC-UV | GLY | 5000- | 35000 | - | 98.5-103 | [ |
Peach field soil (loess soil, black soil and | yes | HPLC-MS/MS | GLY | 1- | 2000 | 10 | 76.7-93.0 | [ |
red soil) | AMPA | |||||||
Yellow cinnamon soil, lou soil and loess soil | yes | HPLC-MS/MS | GLY | 1.6- | 200 | 0.80 | 84.0-104 | [ |
(organic matter content from 0.74%-1.25%) | AMPA | 1.6- | 200 | 0.94 | 84.0-104 | |||
Red loam soil, rice soil and black soil | yes | HPLC-FLD | GLY | 10- | 500 | 20 | 68.3-109 | [ |
- | no | IC | GLY | 20.0- | 1000 | 40 | 80.2-86.4 | [ |
GLUF | 20.0- | 1000 | 80 | 87.1-101 | ||||
AMPA | 5.0- | 400 | 20 | 85.8-106 | ||||
- | no | UPLC-MS/MS | GLY | 20- | 200 | 0.5 | 79.7-96.2 | [ |
AMPA | 20- | 200 | 0.6 | 77.8-99.5 | ||||
- | no | UPLC-MS/MS | GLY | 100- | 10000 | 100 | 85.8-94.6 | [ |
- | no | UPLC-MS/MS | GLY | 10- | 1000 | 20 | 77.5-92.0 | [ |
AMPA | 10- | 1000 | 20 | |||||
GLUF | 5- | 500 | 10 | |||||
Peach field soil (organic matter content | no | UPLC-MS/MS | GLY | 5- | 500 | 4.0 | 74.2-78.8 | this |
2.89%-7.38%) | AMPA | 83.7-91.2 | method | |||||
GLUF | 2- | 500 | 2.0 | 94.1-101 | ||||
MPP | 97.5-104 | |||||||
NAG | 94.4-108 |
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